Method for producing (1S,2R)-2-chloro-2-fluorocyclopropanecarboxylic acid
a technology of cyclopropanecarboxylic acid and method, which is applied in the preparation of carboxylic acid esters/lactones, organic chemistry, and carboxylic compound preparations. it can solve the problems of low yield and selectivity of the method disclosed in ptl 1 and achieve high yield, sufficient selectivity, and high yield
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production example 1
[0130]Under a nitrogen atmosphere, 318 g of water, 188 g (1.35 mol) of glycine ethyl ester hydrochloride, and 188 g of n-heptane were sequentially supplied, and the resulting mixture was then cooled to 10° C. To the mixture, 1.74 g of 28 weight % sodium hydroxide aqueous solution was added to adjust its pH to 4.7. While keeping the internal temperature at 10±2° C., 279 g of 40 weight % sodium nitrite aqueous solution (net: 112 g, 1.62 mol) and a citric acid aqueous solution containing 4.54 g (0.0216 mol) of citric acid monohydrate and 65.8 g of water were simultaneously added dropwise over a period of 3 hours to the mixture obtained above. The resulting mixture was kept at 10° C. for 6 hours, and a sodium carbonate aqueous solution containing 6.58 g (0.0621 mol) of sodium carbonate and 87.5 g of water was added to the mixture dropwise. The mixture thus obtained was subjected to liquid-liquid separation wile maintaining the internal temperature at 10±5° C. The organ...
production example 2
[0131]Under a nitrogen atmosphere, 212 g of water, 126 g (0.900 mol) of glycine ethyl ester hydrochloride, and 126 g of n-hexane were sequentially supplied, and the resulting mixture was then cooled to 10° C. To the mixture, 1.99 g of 28 weight % sodium hydroxide aqueous solution was added to adjust its pH to 4.9. While keeping the internal temperature at 10±2° C., 186 g of 40 weight % sodium nitrite aqueous solution (net: 74.5 g, 1.08 mol) and a citric acid aqueous solution containing 3.03 g (0.0144 mol) of citric acid monohydrate and 43.9 g of water were simultaneously added dropwise for a period of over 2 hours to the mixture obtained above. The resulting mixture was kept at 10° C. for 7 hours, and a sodium carbonate aqueous solution containing 4.39 g (0.0414 mol) of sodium carbonate and 58.3 g of water was added to the mixture dropwise. The mixture thus obtained was subjected to liquid-liquid separation wile maintaining the internal temperature at 10±5° C., obt...
production example 3
Distillation of Ethyl Diazoacetate
[0132]A n-hexane solution of ethyl diazoacetate obtained in Production Example 2 (213 g, content: 41.0 weight %, net: 87.2 g) was concentrated at a temperature of 38° C. to 42° C. and a reduced pressure of 200 hPa to 370 hPa. The resulting residue was subjected to distillation at a temperature of 52° C. to 60° C. and a reduced pressure of 12.0 hPa to 31 hPa, obtaining 70.1 g of ethyl diazoacetate (content: 96.5 weight %, net: 67.7 g) in the form of a yellow oily substance.
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